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2007 Vol. 27, No. 08
Published: 2007-08-26
 
       光谱学与光谱分析
1457 Time-Resolved Terahertz Spectroscopy of Explosives
ZHANG Liang-liang1,2,ZHANG Cun-lin2,ZHAO Yue-jin1,LIU Xiao-hua1
The authors present a time-resolved measurement in terahertz (THz) frequency region by means of the free-space electro-optic sampling (FSEOS). The transmission spectra and complex refractive index of four kinds of explosives were obtained. The authors found that DNT, RDX, HMX and TNT all have absorption peaks within the frequency range of 0.2 and 2.5 THz. It can be seen that DNT and HMX have obvious absorption peaks at 1.08 and 1.82 THz respectively. The authors can use the terahertz spectra as the fingerprint of the detected materials. Therefore, time-resolved terahertz spectroscopy can be applied to detect and identify explosives. The authors also detected a kind of carcinogen named azobenzene. The authors found that azobenzene bought both in China or from American all have the absorption peaks in the frequency range between 0.2 and 2.5 THz.
2007 Vol. 27 (08): 1457-1460 [Abstract] ( 2471 ) PDF (1328 KB)  ( 572 )
1461 A New Parameter for Evaluating Spectral Estimation Precision of Multispectral Camera
LI Sui-xian,LIAO Ning-fang,SUN Yu-nan
The present paper is related to the problem of evaluating the spectrum estimation precision of multispectral imaging camera. First, the definition of index of shifting degree(ISD) is given mathematically. Then, a new method, the index of system spectrum estimation shifting degree(ISSD), to evaluate the spectral match ability of multispectral camera is proposed. Both of them use only one index to evaluate the match degree of spectrum curve pairs and the spectrum estimation performance of multispectral camera(system) quantitatively. The feasibility of the newly advanced index is verified via numerical calculation, with the data of 24 typical spectrum pairs and that of 17 intended designed multispectral cameras′ simulation results. The results of numerical calculation of the parameter also indicated that the ISSD may be served as a criterion to classify multispectral cameras with different spectrum estimation performance.
2007 Vol. 27 (08): 1461-1464 [Abstract] ( 1991 ) PDF (1257 KB)  ( 510 )
1465 Variation of Spectral Response Curve Shape of GaAs Photocathodes
ZOU Ji-jun1,2,CHANG Ben-kang1*,DU Xiao-qing1,YANG Zhi1
Using spectral response measuring instrument, the spectral response curves of reflection-mode GaAs photocathodes were obtained as a function of time during the process of activation and the process of illumination by white light after activation. The measured results show that the spectral response curve shape changes continuously during both processes. Due to the formation of double dipoles on the GaAs surface during the co-adsorption of cesium and oxygen, the surface electron affinity of photocathode decreases continuously, and spectral response increases continuously, but the spectral response of long wave increases faster. During the process of illumination by white light after activation, due to the double-dipole structure affected by the desorption of cesium, the surface electron affinity of photocathode increases continuously, and spectral response decreases continuously, but the spectral response of long wave decreases faster. Using traditional quantum efficiency formula of reflection-mode photocathodes, the above phenomena cannot be explained very well, and they have a relationship with the escape of high-energy electrons. Because the emitted electron energy-distribution of reflection-mode photocathodes shifts towards higher energies with the increase in photon energy, and the influence of the evolution of surface potential barrier profile on the low-energy electrons is greater, the spectral response curve shape changes during different processes.
2007 Vol. 27 (08): 1465-1468 [Abstract] ( 1654 ) PDF (800 KB)  ( 504 )
1469 The Resonance-Enhanced Ionization Spectrum of NO via (3+1) Multiphoton Process
ZHANG Gui-yin,JIN Yi-dong
The resonance-enhanced multi-photon ionization (REMPI) spectrum of NO in the region of 420-500 nm was obtained with the optical parameter generator and amplifier pumped by a Nd∶YAG laser as the radiation source. The spectrum presents the characteristic of banded structure. This indicates that NO molecule is ionized in a resonant manner and via a multi-photon process in this wavelength region. The fact that the variation of the ion signal intensity versus the laser intensity is near quartic suggests that the NO molecule is ionized by a four-photon process. Based on the theoretical calculation,a spectral progression that comes from the (3+1) multiphoton process and via E 2Σ intermediate resonant state is ascribed. The ionization pathway of NO molecule can be expressed as NO(X 2Π)3hν→NO(E 2Σ)hν →NO++e. The vibration constants of NO E 2Σ state were obtained from analyzing the result. So the study of the energy level structure of NO E 2Σ state by the technique of REMPI was realized for the first time.
2007 Vol. 27 (08): 1469-1472 [Abstract] ( 1100 ) PDF (752 KB)  ( 419 )
1473 Effect of Substrate Temperature on Optical Emission Spectra in Electron-Assisted Chemical Vapor Deposition of Diamond
WANG Zhi-jun,LI Pan-lai,SHANG Yong,HE Ya-feng,RAN Jun-xia
The optical emission spectra of atomic hydrogen (Hα,Hβ and Hγ),atomic carbon C(2p3s→2p2: λ=165.7 nm) and radical CH(A2Δ→X2Π: λ=420-440 nm) in the gas phase process of the diamond film growth with electron-assisted chemical vapor deposition (EACVD) from a gas mixture of CH4 and H2 were studied by using Monte-Carlo simulation. The effects of substrate temperature on the optical emission spectral and diamond synthesis were investigated. The results showed that the range of variation of intensities of optical emission spectra near the substrate with the substrate temperature is wider than that far from the substrate,suggesting that the substrate temperature just affects the gas phase reaction process near the substrate,and the strong dependence of the quality of diamond film on the substrate temperature is due to the change in phase process near the substrate brought by the substrate temperature.
2007 Vol. 27 (08): 1473-1475 [Abstract] ( 1271 ) PDF (568 KB)  ( 527 )
1476 Confirmation of Optimal Excitation and Emission Wavelengths Based on Indicator Kriging Method
HE Qing-hang,ZHANG Zhen-xi*,WANG Jing
Excitation wavelength and emission wavelength are vital parameters of molecular fluorescence spectral measurement,whose choice influences the precision of molecular fluorescence spectral measurement and its subsequent study. Because measurement precision of some spectral instrument such as fluorescence spectrometer HITACHI F-4500 can not reach the requirement of spectral analytical technique,and the measurement data is finite,in practical work,the required data are obtained from measurement data using interpolation,which becomes an effective solving method. Therefore,the present paper studies the confirmation of certain volume percentage ethanol solution′s optimal excitation wavelength and optimal emission wavelength using indicator Kriging method: the optimal excitation wavelength and optimal emission wavelength based on indicator Kriging method are 226.9 and 337.1 nm respectively,with verification. Furthermore,the interpolation result is valuated using relative standard deviation. These results indicate that it is feasible to confirm the optimal excitation wavelength and optimal emission wavelength based on indicator Kriging method in the molecular fluorescence spectral measurement,which supplies a novel method for the confirmation of optimal excitation wavelength and optimal emission wavelength.
2007 Vol. 27 (08): 1476-1479 [Abstract] ( 398 ) PDF (689 KB)  ( 479 )
1480 Photoluminescence Properties of Europium-Terbium-Gadolinium-Hexafluoroacetylacetone Ternary Complexes Synthesized in-situ in Gel Glass
HU Quan2,SHENG Xia1,LIU Si-qian1,ZHANG Yan1,QIAN Guo-dong1*
The luminescence property of the inorganic glass doped with rare earth complex has aroused a wide range of attention for a variety of technological applications such as optical devices,biomedicine,etc. In the present work,the ternary complexes of europium-terbium-gadolinium with hexafluoroacetylacetone (HFA) and triphenylphoshine oxide (TPPO),Eu1/2-xTb1/2-xGd2x(HFA)3(TPPO)2 (x=0 or 1/18),were synthesized in-situ in gel glasses to obtain transparent materials. The photoluminescence (PL) spectra were measured and the characteristic transitions of Eu3+ and Tb3+ observed. Due to the phonon assisted energy transfer between Gd3+ (bonding ligands),Tb3+ and Eu3+,the intensity ratios of europium luminescence band to terbium band vary remarkably with the measurement temperatures. In addition,the Frster mechanism has proven responsible for the energy transfer between Eu3+ and Tb3+. The complex-doped gel glass whose luminescence color changes with temperatures is promising for being used as temperature detector,biological probe and thermal-sensitive probe of optical fiber sensor.
2007 Vol. 27 (08): 1480-1483 [Abstract] ( 1157 ) PDF (1150 KB)  ( 474 )
1484 Application of Digital Fourier Filtering Pretreatment Method to Improving Robustness of Multivariate Calibration Model in Near Infrared Spectroscopy
LI Qing-bo1,ZHANG Guang-jun1*,XU Ke-xin2,WANG Yan2
In the application of near infrared spectral analysis,it often occurs that the multivariate calibration model can only predict accurately the samples whose measuring conditions are the same as those of the training set. When the measuring conditions of the predicted samples change,the calibration model would predict the measured samples with greater prediction errors. In the present paper,digital Fourier filtering pretreatment method was used for the glucose aqueous solution temperature experiments. Experiment 1 was carried out at constant 25 ℃,while experiment 2 at constant 30 ℃. Experiment 3 was performed at ambient temperature. Samples of experiment 1 and experiment 2 were employed as the training set to optimize the calibration model. And then the samples of experiment 3 were used as the validation set to evaluate the prediction error of the model. The results showed that the root mean square of prediction error (RMSEP) of the validation set was 664.47 mg·dL-1 for the partial least squares (PLS) calibration model without digital Fourier filtering pretreatment,while the RMSEP of the validation set was reduced to 58.43 mg·dL-1 for the PLS calibration model with digital Fourier filtering pretreatment,and the correlation coefficient between prediction values and reference values increased. It is showed that the digital Fourier filtering pretreatment method could improve robustness of the multivariate calibration model.
2007 Vol. 27 (08): 1484-1488 [Abstract] ( 1853 ) PDF (1127 KB)  ( 543 )
1489 Study on the Influence of Resolution on Near Infrared Spectra and Quantitative Analysis
XIE Li-juan,LIU Dong-hong*,ZHANG Yu-huan,XU Hui-rong,YE Xing-qian,YING Yi-bin
Near-infrared (NIR) spectroscopy technique is one of the qualitative and quantitative analysis techniques that were developed quickly in recent years.NIR spectroscopic analyses are non-destructive,simple and fast,and require no sample pretreatment,which makes this technology ideally suited for on line process monitoring and quality control. As a powerful analytical tool in product quality determination,this technology is based on the measurement of the frequencies of vibrations of chemical bonds in functional group such as C—C,C—H,O—H,CO and N—H upon absorption of radiation. A good and robust model is very important for NIR spectroscopy analysis. However,it was found that the status of NIR spectrometer and the set of parameters when scanning,such as accuracy of wavelength,resolution of apparatus,noise,scan time and uniformity of sample size,had effect on the spectrum quality. In the present paper,NIR transmittance spectra of bayberry juice were obtained and quantitative analysis was carried out. The influence of resolution on the NIR spectra and quantitative models was studied. Forty three bayberry samples with different varieties and ages were used in this experiment. Cross-validation was used to develop models and evaluate and compare these models. The results show that resolution does have effect on the NIR spectra and quantitative models. The spectrum with high resolution was rougher than that with low resolution. Moreover,the scan speed was lower and more data size was required when high resolution was used. The difference in root mean square noise and mean absorbance at different resolutions was distinct (α＝0.05). The best acid model was developed with 4 cm-1 spectral resolution,giving the relative high correlation coefficient of 0.994 04,and a root mean square error of calibration (RMSEC) and root mean square error of cross validation (RMSECV) of 0.023 3 and 0.153,respectively. However,if no information was lost,a resolution of 8 cm-1 was suggested considering the scanning time and data size.
2007 Vol. 27 (08): 1489-1492 [Abstract] ( 2027 ) PDF (589 KB)  ( 454 )
1493 Study on Quality Control of Traditional Chinese Medicine Ginseng Injection with Fourier Transform Infrared Spectroscopy
CHEN Jian-bo1,ZHOU Qun1,SUN Su-qin1*,YU Lu1,XU Kang-ya2
Three kinds of traditional Chinese medicine injection samples were systematically studied via FTIR spectroscopy combined with second derivative and 2D correlation IR spectroscopy. Comparison was successfully made among different kinds and batches of the medicine samples. In conclusion,the multi-steps IR macro-fingerprint method was demonstrated to be a rapid,simple and reliable method in the quality control of traditional Chinese medicine injection.
2007 Vol. 27 (08): 1493-1496 [Abstract] ( 478 ) PDF (2253 KB)  ( 498 )
1497 Wavelet-Transform Based Identification of Ginseng of Different Ages Using Two-Dimensional Infrared Correlation Spectroscopy
ZHAN Da-qi1,CHEUNG Yiu-ming2,SUN Su-qin1*
Wavelet transform was applied to the pretreatment of dynamic spectra data of two-dimensional infrared correlation spectroscopy. The results showed that with the pretreatment,the resolution of synchronous spectrum was noticeably improved. The peaks in the spectrum were toned up,and were separated from each other much more clearly than before. All these enhanced the performances of two-dimensional infrared correlation spectroscopy in analyzing and identifying complicated system. With this approach,ginseng of different ages can be identified.
2007 Vol. 27 (08): 1497-1501 [Abstract] ( 1818 ) PDF (2116 KB)  ( 505 )
1502 Spectral Characteristics and Their Correlation with Soil Parameters of Black Soil in Northeast China
SUN Jian-ying,LI Min-zan*,TANG Ning,ZHENG Li-hua
The spectral characteristics of black soil in northeast China were studied,and the difference of the characteristics was discussed between the black soil and the grey-brown alluvial soil in northern China. Results showed that the spectral characteristics of the two types of soil with higher moisture content were very alike,while the NIR absorbance spectra and the first derivative spectra of the two types of soil exhibited great difference with lower moisture content. The possible reason was the influence of soil texture. The correlation analysis between the main soil parameters and NIR absorbance spectra of raw soil samples was conducted. There was a high correlation between soil moisture content and absorbance spectra. And correlation was observed between soil TN(total nitrogen) and absorbance spectra. However,it was not observed for soil organic matler(SOM) since SOM of black soil in northeast China was higher,and the spectral absorbance of SOM attained saturation.
2007 Vol. 27 (08): 1502-1505 [Abstract] ( 1142 ) PDF (485 KB)  ( 468 )
1506 Study on the Phase Shift Error of the Dynamic Spectrum
WANG Yan1,2,LI Gang1*,LIN Ling1,LIU Yu-liang1
Dynamic spectrum (DS) is a kind of NI spectrum extracted from the photo-electric pulse wave and closely relative to the article blood. It can be used in a non-invasive blood component concentration examination decision. In the present paper,the phase shift error (PSE) in the DS detection is analyzed based on the measure theory of DS. Firstly,the physiological activity of human being results in the instability of the period,amplitude and the base line of pulse wave. Secondly,there is a phase shift between different pulse waves at different wavelengths during the detection in time domain. These two factors lead to the difference among different pulse waves,and introduce the PSE into DS. The PSE of DS among different pulse waves is also discussed quantitatively. The result showed that PSE is correlated with the position of the rectangle window that intercepts pulses from the wave,and can be minimized into about 10% by selecting the start points of the windows.
2007 Vol. 27 (08): 1506-1509 [Abstract] ( 1511 ) PDF (857 KB)  ( 480 )
1510 Study on the Reaction Mechanism of Surface Modified Nano-CaCO3 Particles Using w-Undecenoic Acids as Modifier by FTIR Difference Spectroscopy
CHU Yan-hong1,2,ZHANG Guo-bao2,ZHAO Gen-suo2,YU Shou-zhi2,WANG Jing-wu1*,LI Bin-jie3
The components of the surface modified nanometer calcium carbonate particles with w-undecenoic acids as modifier were tested by differential FTIR spectroscopy. Some special absorption bands respectively assigned to (RCOO)2-Ca,γC—CH,νC—CH,νRCOOR,νRCOOH at the wavenumbers of 1 572,1 542,912,3 078 cm-1,1 746 and 1 703 cm-1 were found. The possible modification mechanisms is that the organic acid reacts with the exposed Ca2+ of the nano-CaCO3 surface to form ion-bond (RCOO)2Ca;and the other organic groups are absorbed onto the surface of nano-CaCO3 by hydrogen-bond. These organic groups twist on the surface of nano-CaCO3 particles. So the dispersion of the modified nano-CaCO3 particles is increased remarkably in absolute ethanol.
2007 Vol. 27 (08): 1510-1513 [Abstract] ( 1852 ) PDF (914 KB)  ( 507 )
1514 An Outlier Diagnosis on Near Infrared Spectroscopy Analysis of NDF Content in Corn Silage Feeds
LIU Qiang1,LUO Chang-bing2,CHEN Shao-jiang3,MENG Qing-xiang1*
An experiment was conducted to study the outlier diagnosis on the near infrared spectroscopy (NIRS) analysis of NDF content in corn silage feeds. Various Mahalanobis’ distances including 3 and 2×Mahalanobis’ distances and the average of Mahalanobis’ distance +2 SD (AV+2 SD) were set to diagnose the spectral outliers during the model development,and their effects on the calibration models were compared respectively. The results showed that it was feasible to diagnose the spectral outliers for NIRS analysis of NDF content in corn silage feeds when the Mahalanobis’ distance was AV+2 SD,the r is 0.97 and the SEC is 2.456. The calibration model optimized under such conditions was the best.
2007 Vol. 27 (08): 1514-1518 [Abstract] ( 638 ) PDF (1150 KB)  ( 484 )
1519 Identification of Fusarium by Fourier Transform Infrared Spectroscopy
NIE Ming1,LUO Jiang-lan1,BAO Kan1,ZHANG Wei-qiong1,YANG Shi-ping1,XIAO Ming1,2*,LI Bo2
Fourier transform infrared (FTIR) spectroscopy,in combination with multi-variate statistics,has been a novel tool to identify and classify microorganisms in recent years. In the present study,Fourier transform infrared spectroscopy was used to identify Fusarium belonging to F. oxysporum,F. moniliforme,F. graminearum,F. semitectum,and F. nivale. Distinct spectral differences among these strains were observed from their high-resolution and well-reproducibility infrared spectra in the frequency regions of 3 000-2 800 cm-1,1 800-1 600 cm-1,and fingerprint region. According to the characteristic bands in these regions,different Fusarium species could be identified. And identification by hierarchical cluster analysis was more scientific and reasonable and it also presented a degree of comparability among these strains. But the result was not becoming on reflecting the characteristic of cladistics. FTIR shows high potential as a rapid,accurate and easy-to-use method for the identification of microorganisms. It will be an important tool in microbiological studies.
2007 Vol. 27 (08): 1519-1522 [Abstract] ( 1370 ) PDF (958 KB)  ( 497 )
1523 Analysis of Crop Nutrient Element Potassium in Organic Fertilizer with Near Infrared Spectroscopy Technology
LI Zi-gang1,2,LIU Hao3,QU Ling-bo3*,XIANG Bing-ren2
Potassium in organic fertilizer can be determined by near infrared (NIR) spectral technique,because the spectra are related to the organic groups with NIR absorption. A method for the determination of potassium iron (K+) in organic fertilizer samples was established based on the combination of discrete wavelet transform (DWT) and NIR technique. In the proposed method,the raw NIR data and their wavelet coefficients are used for modeling and prediction of the contents of potassium in organic fertilizer by partial least square (PLS) method. It is shown that there is almost no loss of spectral information with the NIR data compressed to 3.6% of its original size. The model based on wavelet coefficients is better than that based on the full NIR spectral range. With the improved method,accurate prediction can be achieved.
2007 Vol. 27 (08): 1523-1526 [Abstract] ( 2320 ) PDF (856 KB)  ( 522 )
1527 Determination of Berberine in Phellodendron Chinese Schneid from Sichuan Using Near Infrared Diffuse Reflectance Spectroscopy
ZHOU Min1,WANG Tian-zhi1,YE Li-ming1*,CHEN Cong1,HUANG Guo2,WU Yan-wei2
The objective of the present study was to develop a method for the determination of berberine in phellodendron chinese schneid from Sichuan using near infrared diffuse reflectance spectroscopy. Near infrared spectra (NIR) in the range of 12 500-3 600 cm-1 were recorded for the phellodendron chinese schneid containing berberine in the content of 2.155%-8.245% of berberine. Calibration models were established using the PLS (partial least squares). Different spectra pretreatments methods were compared. The study showed that spectra information can be extracted thoroughly by second derivative pretreatments method with the correlation coefficient(r2) of 0.922 1,SEC 0.337 (standard deviation of the calibration sets) and SEP 0.251 (standard deviation of the prediction sets). Results indicated that near infrared diffuse reflectance spectroscopy method can be used to rapidly analyze the valid component in Chinese herbs.
2007 Vol. 27 (08): 1527-1530 [Abstract] ( 2457 ) PDF (824 KB)  ( 513 )
1531 Research on Automobile Speed Identification System with Modulated Infrared Ray
FU He-ping1,WANG Ai-fang2,ZHANG Shuan-ji1,NING Min-dong1,ZHU Jing-cheng1
In order to manage the traffic well and eliminate traffic safety hidden troubles in traffic safety,the way of detecting speed with radar (Doppler effect) is usually adopted to identify and sample speed of illegally running automobile (too fast or too slow). However,another wireless receiving equipment,called electric dog,appears in the recent market. Installed in the automobile,the system can help capture the radar speed detecting signal and an alarm signal will be produced when the automobile approaches the radar detection areas,then the automobile will turn to normal run and escape the traffic management. Once the automobile has passed the radar detection areas,it can run illegally again and the danger still exists. To prevent this circumstance,a new speed identification system with infrared sensor has been developed. It can not only identity the speed,but also show how much it exceeds (+ΔV) or lags (-ΔV) the speed limits. According to the information,it can drive the sampling system to work (to print or take pictures). This way the traffic management can be strengthened effectively,minimizing hidden accidents.
2007 Vol. 27 (08): 1531-1534 [Abstract] ( 2187 ) PDF (978 KB)  ( 452 )
1535 Study on Rapid and Nondestructive Analysis of Danshen Formula Particles by FTIR
WU Jing,SUN Su-qin*,ZHOU Qun,YU Lu
The authors applied Fourier transform infrared (FTIR) spectra to research the quality control of Danshen formula particles manufacturing process and to analyse formula particles from different pharmaceutical factories. The authors can confirm the sort and relative content of supplementary materials by the characteristic absorption peaks of sugar in the range from 1 160 to 1 000 cm-1. The intensity of absorption peaks becomes stronger when the relative content of supplementary materials is higher. The authors can evaluate the relative content of effective component in danshen formula particles by the characteristic absorption peaks at 1 608 cm-1. The intensity of absorption peaks becomes stronger when the relative content of the effective component is higher. FTIR spectrometry is an effective and fast method not only for the quality control of Danshen formula particles,but also for identifying the manufacturing technics.
2007 Vol. 27 (08): 1535-1538 [Abstract] ( 2552 ) PDF (1211 KB)  ( 531 )
1539 Study on Quality Control of Safflower Injection and Wild Chrysanthemum Injection with Fourier Transform Infrared Spectroscopy
ZHANG Peng1,SUN Su-qin1*,ZHOU Qun1,XU Kang-ya2
Traditional Chinese medicine (TCM) is a cherishable treasure in the authors’ national culture. Along with the development of scientific technique,the effective ingredient of TCM has been distilled out as a sort of injection that features unique function in emergent first aid compared with other injections. Therefore,people also focus on its security and quality concerns. The experimentation adopts Fourier transform infrared spectroscopy and 2D-IR spectroscopy technique to analyze the injection of safflower and wild chrysanthemum for the purpose of identifying various groups of injection’s quality at first stage.
2007 Vol. 27 (08): 1539-1542 [Abstract] ( 1796 ) PDF (2131 KB)  ( 500 )
1543 Discrimination of Varieties of Cola Using Visual-Near Infrared Spectra
QIU Zheng-jun,LU Jiang-feng,MAO Jing-yuan,HE Yong*
A new method was developed to fast discriminate the brands of cola by means of visual-near infrared spectroscopy (NIRS). Three different brands of cola (Coca-cola,Pepsi-cola and Future-cola) were analyzed using a handheld near infrared spectrometer produced by ASD Company. Fifty five samples were used for each brand of cola,and they were divided randomly into a group of 150 samples as calibrated samples and one of 15 samples as prediction samples. The samples data were pretreated using average smoothing and standard normal variable method,and then the pretreated spectra data were analyzed using principal component analysis (PCA). The principal component data of calibrated samples were used as the inputs of back-propagation artificial neural network (ANN-BP),while the values of cola brands used as the outputs of ANN-BP,and then the three layers ANN-BP discrimination model was built. The 15 unknown prediction samples were analyzed by the ANN-BP model. The result showed that the distinguishing rate was 100%;it was realized to discriminate different brands of Cola rapidly and exactly.
2007 Vol. 27 (08): 1543-1546 [Abstract] ( 2673 ) PDF (1451 KB)  ( 564 )
1547 In situ Temperature-Dependent Raman Spectroscopic Studies on Methane Hydrate Forming in Natural Fluid Inclusion
CHEN Yong,ZHOU Yao-qi
It is always a difficult problem to accurately identify the formation condition of gas hydrates in fluid inclusions in conventional ways. The present paper introduces a new method to get the formation condition of methane hydrate in natural fluid inclusion by in situ Raman spectroscopy. The researched fluid inclusion is in a CH4-H2O system identified by Raman spectroscopy at room temperature. In order to obtain the Raman spectra of methane hydrate,the experimental temperature was controlled in three ways,and the Raman spectra of methane hydrate and ice were obtained at -170 ℃ in the third way. The results of in situ Raman spectroscopy show that the temperature of methane hydrate forming in the authors’ interested inclusion is 7.5 ℃. According to the equilibrium between water and methane hydrate in the CH4-H2O system,the authors’ computed the pressure for the methane hydrate formation to be 5.587 3 MPa. The authors study shows that the in situ Raman spectroscopy is an effective method to obtain the formation condition of gas hydrates in fluid inclusions.
2007 Vol. 27 (08): 1547-1550 [Abstract] ( 1260 ) PDF (919 KB)  ( 531 )
1551 Study on the Spectra of Spruce Lignin with Chlorine Dioxide Oxidation
SUN Yong1,2,ZHANG Jin-ping1,2,YANG Gang1,2,LI Zuo-hu1
The Fourier transform infrared spectroscopy (FTIR),ultraviolet-Visible spectroscopy (UV-visible),Fourier transform Raman spectroscopy (FT-Raman),and nuclear magnetic resonance spectroscopy (1H NMR) were used to study the oxidation of spruce lignin by chloride dioxide. The results are as following: The selective oxidation of lignin by chlorine dioxide was obtained by spectroscopy study. FTIR showed that the characteristic absorbance peak of guaiacyl unit in the lignin structure was decreased after chloride dioxide oxidation,while the peaks of syringyl and para-hydroxyphenol disappeared after oxidation. The largely increased absorbance for the band around 1 720 cm-1 corresponding to carbonyl stretching was achieved in the oxidized lignin. The ultraviolet-visible spectroscopy showed that the absorbance around 280 nm was largely reduced after the lignin had been oxidized. The 1H NMR spectroscopy also showed the decrease of aromatic units and methoxyl group in the oxidized lignin. These indicated the formation of ester,or quinone derivatives when the lignin was selectively oxidized by chloride dioxide.
2007 Vol. 27 (08): 1551-1554 [Abstract] ( 2134 ) PDF (988 KB)  ( 521 )
1555 Effects of Silver Nanoparticles on Fluorescent Properties of Fluorescein
WANG Yue-hui,ZHOU Ji*,WANG Ting
The effects of silver nanoparticles on the fluorescent properties of the fluorescein in aqueous solution were investigated in the present paper. The fluorescein-coated silver nanoparticles form Fln-Ag complexes,leading to a net-like structure among silver nanoparticles. The fluorescent intensity of the fluorescein was enhanced due to the energy transfer from silver nanoparticles to fluorescein owing to the local field enhancement brought by the surface plasmon resonance of silver nanoparticles. Furthermore,with the increase in silver nanoparticle concentrations the fluorescence enhancement efficiency has a maximum. The larger-size silver nanoparticles have a maximum enhancement efficiency in the lower concentration region. The energy transfer between the fluorescein and silver nanoparticles depends on the local field enhancement around the fluorescein,the nonradiative energy transfer,the silver nanoparticles concentration and size.
2007 Vol. 27 (08): 1555-1559 [Abstract] ( 1352 ) PDF (1569 KB)  ( 560 )
1560 Study on the pH Induced Conformational Change of Plant CaM by Using Tb3+ Luminescence Probe
XIAO Feng-juan1,CHANG Hong2,LIU De-long３
Calmodulin(CaM) is a ubiquitous Ca2+binding protein of eukaryotes,and regulates a broad spectrum of fundamental cellular processes. It has been established that CaM has both intracellular and extracellular signal transduction functions,but the mechanism of the fact that extracellullar CaM can be activated by Ca2+ has been unclear. In order to establish the binding parameters of Ca2+ to extracellular CaM at high Ca2+level and low pH,Tb3+ fluorescence probe and fluorescence spectroscopy were used to investigate the influence of pH values on the conformational change of plant CaM. The fluorescence spectra in apo-CaM had blue shift and were quenched along with the change of pH value from 7.0 to 2.0. The fluorescence intensity of Ca-CaM system was remarkably lower than that of the Tb-CaM system and the Tyr-sensitized Tb3+ fluorescence in Tb3+-CaM was quenched with the addition of H+. On the basis of the results the relation between fluorescence intensity and conformational change of plant CaM and the mechanism of the changes in Tyr microenvironment induced by pH were discussed. It can be assumed that H+ can not only bind to CaM competiting with Ca2+ or Tb3+ but also alter the hydrophobic environment on the surface of CaM molecules,which may affect the activity of CaM. The study supports the extracellular CaM signal transduction mechanism significantly.
2007 Vol. 27 (08): 1560-1564 [Abstract] ( 526 ) PDF (1324 KB)  ( 483 )
1565 A New Method for Chemical Analysis: Fluorescence Capillary Analysis
LI Yong-sheng1,GAO Xiu-feng2*
A new analytical approach called fluorescence capillary analysis (FCA) has been proposed. FCA method uses a capillary as a carrier for fluorescence reaction and determination,and with this method micro analysis of micro samples has been realized. Its advantages are simple to manipulation,thimbleful of sample and reagent volumes (＜10 μL),repeated use of capillary,and the lowest test cost. FCA method can consumedly decrease the pollution of the environment. Based on FCA and an immobilization enzyme FCA,VB2,NADH,and ethanol in alcohol drinks have been determined. Based on an immobilization probe gene FCA,target nucleotide also has been determined. These results were satisfactory. FCA method can be used for fermentable food,medicine,biochemistry,industry,etc.
2007 Vol. 27 (08): 1565-1569 [Abstract] ( 867 ) PDF (980 KB)  ( 430 )
1570 Determination of 8-Hydroxy-2’-Deoxyguanosine in Urine with Protamine Using Resonance Energy Transfer Fluorescence Quenching by Sensitizing Effect of Triton X-100
MI Xian-wen1,3,WANG Yong-sheng1,2*,XUE Jin-hua1,OUYANG Yun-fu1,YANG Sheng-yuan1,WANG Ying1
The optimum conditions for the resonance energy transfer between 8-hydroxy-2’-deoxyguanosine(8-OHdG) and protamine were studied,and a novel method for the determination of 8-OHdG has been developed based on the resonance energy transfer fluorescence quenching effect of protamine. The fluorescence quenching intensity of Ps at 301 nm was proportional to the concentration of 8-OHdG. The linear range of the calibration curve was 0.50-7.1 μg·mL-1 in the pH 8.2 Tris-HCl buffer solution with the detection limits of 0.18 μg·mL-1. The relative standard deviation was 6.2% and the average recovery was 104%(n=6). The proposed method is simple and sensitive,and has succeeded in analyzing the spiked urine sample with satisfactory results.
2007 Vol. 27 (08): 1570-1573 [Abstract] ( 1164 ) PDF (762 KB)  ( 426 )
1574 Monitoring Model and Temporal-Spatial Changes of Dissolved Oxygen Based on Remote Sensing: a Case Study in Huangpu River
XIE Huan1,2,TONG Xiao-hua1*,QIU Yan-ling3,ZHANG Hong-en3,ZHANG Ya-lei3,ZHAO Jian-fu3
The concentration of dissolved oxygen (DO) is one of the most important quality indicators to reflect the water organic pollution. In the present paper,the typical water quality parameter in Huangpu River upper region,namely dissolved oxygen (DO),is chosen as the research object. Using ground hyperspectral remote sensing data,multispectral remote sensing data and in situ water quality monitoring data,the relation between the characteristic of water spectral reflectance and the concentration of DO is first analyzed. The result generated with the given monitoring methods indicates that the correlation between DO concentration and spectral reflectance at band 641 nm is the highest,while the logarithmic model using the ratio of Landsat5 TM band 3 to 4 as an independent variable has the highest correlation coefficient (0.829). The accuracy and the generality of the derived model are then tested,and the temporal-spatial changes of dissolved oxygen based on multi-temporal remote sensing imageries are further studied. The result shows that the DO model has a high accuracy,the temporal change characteristic of estimated DO is in consistency with that of measured ground data,and the DO concentration distribution derived from this model is also in accordance with the practical organic pollution distribution characters in this region.
2007 Vol. 27 (08): 1574-1579 [Abstract] ( 219 ) PDF (1729 KB)  ( 553 )
1580 Synthesis and Characterization of Thiaxanthon-2-yl-oxyacetate and Its Combination with ct-DNA
SHEN Shao-bin,ZHENG Xiu-rong,SONG Yu-min*,LU Xiao-lin
The thiaxanthon-2-yl-oxyacetate was synthesized,and its structure was characterized by elemental analysis,IR,1H NMR,and 13C NMR spectra. It was found from the experiment that thiaxanthon-2-yl-oxyacetate had very intense fluorescence,so spectroscopy methods were used to study the interactions of thiaxanthon-2-yl-oxyacetate and ct-DNA. The ultraviolet absorption intensity of thiaxanthon-2-yl-oxyacetate decreased as the concentration of ct-DNA increased at pH 7.38. There was some debased intensity both in the negative and positive spectra of CD spectra of ct-DNA when thiaxanthon-2-yl-oxyacetate interacted with ct-DNA,and quenching effect occurred in the fluorescence spectrum of thiaxanthon-2-yl-oxyacetate. The quenching constant is 1.25×104 L·mol-1,when the concentration of ct-DNA changed from 0 to 12.0 mg·L-1,and the connection between the quenching data and the concentration of ct-DNA shows a favorable linear relationship. The detection limit was 1.63 mg·L-1,so the compound is a new reagent for the measurement of ct-DNA. The interaction of TYO and ct-DNA was insetted and static.
2007 Vol. 27 (08): 1580-1583 [Abstract] ( 2154 ) PDF (787 KB)  ( 453 )
1584 Synthesis and Spectral Study of Amine Salt of Tungstovanadophosphoric Heteropolyacid with Dawson Structure
LIU Xia1,ZHAO Jun2,FENG Chang-gen2*,LI Hong-zhen3
Parent heteropoly salt was prepared by the method of stepwise addition of materials-stepwise acidification and distillation. Firstly,tungstovanadophosphoric heteropolyacid with tri-wanadium-substituted Dawson structure was synthesized with ammonium metavanadate,sodium dihydrogen phosphate and sodium tungstate as materials under the conditions of pH 4 and reaction time of 10 h. Secondly,parent heteropoly salt K9P2W15V3O62·41H2O was prepared by adding counterion K+ 5 times as much as determined by stoichiometric relation of reaction to the solution of tungstovanadophosphoric heteropolyacid. The acid solution of the parent heteropoly salt was slowly added to the solution of hexadecyltrimethylammonium bromide with continually stirring,then amine salt of tungstovanadophosphoric heteropolyacid,(C19H42N)6H3[P2W15V3O62] was synthesized. The target compound was characterized by elemental analysis,IR,XRD powder diffraction and TG-DTA,and the results indicated that it was a new heteropoly compound retaining Dawson structure.
2007 Vol. 27 (08): 1584-1586 [Abstract] ( 1903 ) PDF (554 KB)  ( 477 )
1587 Studies on the Determination of Protein by a New Resonance Rayleigh Scattering System
LIN Xu-cong,WU Meng-hui,GUO Liang-qia,XIE Zeng-hong*
Using 1,6-hexanediaminediacridine as a spectrum probe,a new method of quantitative determination of protein by resonance Rayleigh scattering (RRS) has been developed. Characteristics of the resonance scattering reaction of the acridine probe with bovine serum albumin (BSA) were investigated. Effects of the concentration of acridine probe and pH value of the buffer solution,as well as the stability of the resonance scattering interaction,were also studied,and then the optimum condition was obtained. In the Tris-HCl buffer solution,the intensity of resonance Rayleigh scattering spectrum remained stable without any notable change in the pH range of 6.0-7.5. While pH ranged from 8.0 to 8.9,the interaction of BSA and acridine was accelerated. The resonance scattering was increasing and the peak value was gained at pH 8.9. However,with the augmentation of pH from 10.0 to 11.0 in Na2B4O7-NaOH or Na2HPO4-NaOH buffer medium，some negative effects on the molecular structure and nature of BSA might occur and resulted in a too high background scattering noise,which caused a rapid decrease in the resonance scattering intensity. A good calibration curve of the protein was obtained in the range of 1.00-5.00 μg·mL-1 with a detection limit (3σ/K) of 0.085 μg·mL-1. Applied to the quantitative analysis of BSA simulant samples,the result was satisfied and the recoveries were 98.0%-101.7% at the concentrations ranging from 2.00 to 4.00 μg·mL-1. The relative standard deviation was less than 1.7%.
2007 Vol. 27 (08): 1587-1590 [Abstract] ( 1176 ) PDF (559 KB)  ( 472 )
1591 Study on Degradation and Decolouration of Polycyclic Aromatic Hydrocarbons Crystal Violet by Photo-Fenton Reagent
LI Hong1,LI Xiao-hong1,PENG De-jun3,ZHENG Huai-li2,3*
The crystal violet is one of polycyclic aromatic hydrocarbons. In the present paper,the degradation of the crystal violet by photo-Fenton reagent was studied. Through numerous experiments,the influences of various parameters including the wavelength-absorbency curve of the crystal violet,the concentration-absorbency curve of the crystal violet,the initial pH of solution,the initial concentration of the crystal violet,different irradiation time,the dosage of FeSO4,the dosage of H2O2 and orthogonal experiments were researched intensively. Through numerous experiments，the optimum conditions for crystal violet degradation were given. The main optimum conditions for crystal violet degradation are as follows: The initial optimum pH of solution is 3-4;The optimum concentration of the crystal violet is below 0.080 0 g·L-1. The optimum dosage of H2O2 is 1Qth. The optimum dosage of FeSO4 ranges from one fiftieth to one hundredth of the dosage of H2O2. Under the optimal conditions,the sun light can promote this reaction apparently,the reaction time can greatly be shortened,and the dosage of oxidant and catalyst can be saved too.
2007 Vol. 27 (08): 1591-1595 [Abstract] ( 2402 ) PDF (1299 KB)  ( 453 )
1596 Preparation and Spectral Characteristic of Molecularly Imprinted Polymers for Sulfamethazine
LIU Hui-jun1,XU Wei-jian2,LIU Yao-chi1,XIONG Yuan-qin2
Molecularly imprinted polymers(MIPs) were synthesized,which was initiated by UV photo-induction at low temperature,with sulfamethazine(SM2) was used as template,methacrylic acid(MAA) as monomer,and ethylene glycol dimethylacrylate (EGDMA) as crosslinker. By UV spectrometry the authors compared the combination action on sulfamethazine with MAA and researched the static adsorption ability and selective recognition of the molecularly imprinted polymers. The results showed that the combination action of functional monomer with template molecules was produced,sulfamethazine imprinted polymers using methacrylic acid as monomer had higher affinity capability than NMIP and comparatively similar structure substrate of sulfisoxazole(SIZ),while SM2 imprinted polymers could specifically recognize the corresponding imprinted molecules. The static adsorption modulus of SM2 imprinted polymer was 282.3 mg·mL-1 and the separate factor was 3.9. Then,the prediction imprinting principle of sulfamethazine template polymer was given. The infrared spectra of methacrylic acid (MAA) and ethylene glycol dimethylacrylate (EGDMA) and MIPs of SM2 were analysed. It was found that the absorbability peak of CC function group in the IMPs turned out to be very low,but the function group of carboxylic acid in the IMPs did not markedly change. The results showed that there were some functional groups in MIPs which could interact with the template.
2007 Vol. 27 (08): 1596-1599 [Abstract] ( 581 ) PDF (790 KB)  ( 508 )
1600 Effect of UV on the Absorption Spectra of E.coli Cells
YANG Tian-you1,2,LI Zong-wei1,ZHANG Feng-qiu1,CHEN Lin-hai1,LI Zong-yi1,QIN Guang-yong1*,HUO Yu-ping1
The present article studied the effects of different solutions in sample cavity on the spectra of E.coli. It is shown that the solutions of 2.8 mL distilled water and 0.1 mL LB and 0.1 mL PBS is the best,because it not only supplies good living condition but also has less effect on the spectra of E.coli. And it was found that UV in spectrophotometer has no effect on the mensuration result. On the basis of these studies the absorption spectra of E.coli irradiated by different doses UV were investigated. It is shown that there is a declining-rising-declining phenomenon in the spectra of E.coli with the dose increasing. This reflects the wound healing process of E.coli. Spectroscopic technique is helpful for the study of cell’s wound healing.
2007 Vol. 27 (08): 1600-1602 [Abstract] ( 1288 ) PDF (638 KB)  ( 563 )
1603 Microscopic Hyperspectral Image Study of Normal and Diabetic Retina Tissues of Rats
LI Qing-li1,XUE Yong-qi2,ZHANG Jing-fa3,LIU Zhi1
A microscopic hyperspectral imaging device was used to study the normal and diabetic retinas of rats. The microscopic hyperspectral images of retinas from normal,diabetic and medicative rats were collected and processed. Some transmission spectral curves of outer nuclear layer of retina were extracted and analyzed. The results showed that there are three characteristic spikes in the spectral curves between 400 and 800 nm from the outer nuclear layer,and the heights of the characteristic spikes at 113 band were altered obviously between the normal and diabetic retinas. In addition,the spectral curve of the diabetic retina changes gradually to the normal spectrum curve after treatment by the LCVS1001. The experiment result showed that the microscope hyperspectral imaging device could be used to study the changes in spectrum characters and physical chemistry composition of the diabetic retina.
2007 Vol. 27 (08): 1603-1606 [Abstract] ( 751 ) PDF (1371 KB)  ( 537 )
1607 Theoretical Research on the Effective Backscattering Cross-Section of Voigt Profile HeⅠ 1 083.0 nm
HE Jian,ZHANG Qing-guo,YAN Shu-qing
In the present paper,considering the Lorentz profile caused by collisions,the backscattering cross-section and the effective backscattering cross-section of Voigt profile (the convolution of Gauss profile and Lorentz profile) of He Ⅰ 1 083.0 nm were studied. The HeⅠ 1 083.0 nm is actually a triplet formed by three very close lines,the 1 083.034 nm,the 1 083.025 nm and the 1 082.908 nm,and the curve and peak value of the backscattering cross-section and the effective backscattering cross-section were given. The order is consistent with the predicted order. This result is closer to the actual case than the Gaussian profile,and gives overall and detailed theoretical basic to resonant Lidar to detect the metastable He in thermosphere. The curves and peak values of the backscattering cross-section and the effective backscattering cross-section of HeⅠ 388.9 nm and HeⅠ 318.8 nm were also given,which are smaller than that of the 1 083.0 nm. This is consistent with the experiment results.
2007 Vol. 27 (08): 1607-1610 [Abstract] ( 2379 ) PDF (722 KB)  ( 465 )
1611 Studies on the Interaction of Hemoporphyrin Metalporphyrin and Levo Dopa
LI Wen-juan1,ZHANG Yong2*,YAN Xin-liang2
Levo dopa (L-DOPA) is a prodrug that is converted to dopamine by DOPA decarboxylase and can cross the blood-brain barrier. When in the brain,levo dopa is decarboxylated to dopamine and stimulates the dopaminergic receptors,thereby compensating for the depleted supply of endogenous dopamine seen in Parkinson’s disease. So,Levodopa is a medication used to treat Parkinson’s disease clinically. In the present paper the interaction of hematoporphyrin and levo dopa was studied by fluorescence at different temperature in the quenching experiments. The excitation fluorescence spectrum of levo dopa displayed a peak at 282 nm and that for the emission fluorescence spectrum was at 320 nm in pH 7.4 buffer solution. The intensity of the fluorescence was effectively quenched as the hemoporphyrin concentration increased and the emission spectra blue-shifted with the isosbestic point appearing,indicating that the interaction between hematoporphyrin and levo dopa occurred and a new complex was formed. According to Stern-Volmer equation and Lineweaver-Burk double-reciprocal equation,the thermodynamic parameters,formation constants and some other concerned constants were obtained. The quenching rate constants Kq bigger than 2.0×1010 L·mol-1·s-1 were found. So the kinetic behavior of the reaction between hematoporphyrin and levo dopa was suggested to be static fluorescence quenching model. In addition,with the temperature increasing,the formation constants decreased to some extent. At 25 ℃,ΔG＝-26.58 kJ·mol-1;ΔS＝138.7 J·K-1 and ΔH=14.71 kJ·mol-1.
2007 Vol. 27 (08): 1611-1614 [Abstract] ( 2091 ) PDF (778 KB)  ( 432 )
1615 Fluorescence Spectrometric Determination of Gatifloxacin by Charge Transfer Reaction
AODENG Gao-wa,TAO Yu-long,FAN Hai-yan
A new method for the determination of gatifloxacin (GFLX) has been developed based on the charge transfer reaction between gatifloxacin as the donor and chloranil(TCBQ) as the acceptor by fluorimetry. Experiments show that GFLX has reacted with TCBQ in a mixture of methanol and water at 45 ℃ for 20 min and the complex was formed. The composition ratio was 1∶1. A linear calibration graph was obtained over the GFLX concentration range from 0.19 to 5.6 mg·L-1 with a detection limit of 0.005 6 mg·L-1. The method has been applied to the determination of GFLX in the preparation,the recoveries are 101.1%-103.9%,and the relative standard deviation is 1.0%-1.9%. At the same time we proposed a method for the determination of GFLX in urine by charge transfer-synchronous fluorescence spectroscopy. Beer’s law is obeyed in the range of 0.023-3.4 mg·L-1 of GFLX with a detection limit of 0.003 4 mg·L-1,the recoveries are 93.9%-101.1%,and the relative standard deviation is 1.0%-1.7%.
2007 Vol. 27 (08): 1615-1618 [Abstract] ( 1691 ) PDF (669 KB)  ( 444 )
1619 Compound Support Vector Machines Method with Application in Spctral Analysis
AN Xin1,SU Shi-guang,WANG Tao1,XU Shuo1,HUANG Wen-jiang2,ZHANG Lu-da1*
Support vector classification (SVC) and support vector regression (SVR) are two main issues of support vector machines (SVM). The present paper combined the two issues,that is,first to built SVC model for classification,then to built SVR models for analysis,and thus brought forward compound support vector machines (CSVM). Based on an idea of simulation study,the CSVM algorithm was built and then validated by building a quantitative analysis model using high-spectrum and leaf nitrogen content data of 71 rice samples which were divided into modeling set and forecasting set randomly at the ratio of 51∶16. For 5 random experiments,the average correlation coefficient of predicted values and standard chemical ones by Kjeldahl’s method of leaf nitrogen content was 0.89,and the average absolute error was 0.088,of which the corresponding values produced by traditional method were 0.87 and 0.091 respectively. It was concluded that the prediction precision of CSVM is higher than that of traditional SVM. CSVM provides a new idea for chemometrics quantitative analysis.
2007 Vol. 27 (08): 1619-1621 [Abstract] ( 633 ) PDF (356 KB)  ( 526 )
1622 The Fluorescence Characteristics of Troxerutin in Micellar System and Their Application
MA Hong-yan,ZHANG She-zheng,CHEN Xiao-li,QI Guang-cai,GUO Ying,ZHANG Hu
The fluorescence characteristics of the troxerutin in micellar system were studied. The experiments indicate that troxerutin can creat initial fluorescence in NaAc-HAc buffer solution and the existence of sodium dodecly benzen sulfonate-6(SDBS-6) can enhance the fluorescence signal of troxerutin greatly. A simple and highly sensitive fluorescence method using the micellar system for the trace analysis of troxerutin has been developed. The experimental conditions that influence the fluorescence intensity were investigated and optimized. The optimum experimental conditions are as follows: in pH 5.53 NaAc-HAc buffer solution,the excitation and emission wavelengths are 350.0 and 456.3 nm,respectively,and the concentration of SDBS-6 is 0.25%. The linear range is 1.6×10-6 mol·L-1-8.0×10-10 mol·L-1 with the detection limit of 1.1×10-10 mol·L-1. The RSD is 1.7%(n=11,c=6.0×10-7 mol·L-1),and the recovery is within the range of 98.5%-100.4%. The method has been successfully applied to the determination of troxerutin in tablets and injections. The results are satisfactory.
2007 Vol. 27 (08): 1622-1624 [Abstract] ( 1263 ) PDF (389 KB)  ( 467 )
1625 Determination of Rutin by Flow Injection Chemiluminescence Method
LI Li-jun1,ZHONG Zhao-heng2,FENG Jun2,CHEN Qi-feng2,KONG Hong-xing1,WU Jian-ling2
A new flow injection chemiluminescence method for the determination of rutin was established. The method was based on the chemiluminescence reaction of rutin with cerium (Ⅳ) sulfate in sulfuric acid condition sensitized by rhodamine 6G. Various factors affecting the chemiluminescence intensity of the system were investigated,and the condition of sulfuric acid,cerium (Ⅳ) sulfate and Rhodamine 6G etc was optimized.We have done research on all kinds of possible disturbers in the sample. The possible mechanism of the proposed method was also studied. The method is simple,convenient and sensitive. The linear relationship between the intensity of chemiluminescence and the concentration of rutin is over the range of 1.0×10-7-1.0×10-4 mol·L-1. The detection limit is 8.1×10-8 mol·L-1,the relative standard deviation is 1.5% for 11 measurements of 1.0×10-5 mol·L-1 standard solution. This method has been successfully applied to the determination of rutin in tablets with recoveries between 99.0% and 104.0%.
2007 Vol. 27 (08): 1625-1628 [Abstract] ( 1798 ) PDF (757 KB)  ( 492 )
1629 Application of ICP-MS/ICP-AES to the Detection of Wholesome Elements and Heavy Metals in Soybean from Northeastern China
YAN Ping-mei1,2,WANG Wen-ya3,RUI Yu-kui4*,ZHANG Fu-suo4,JIN Yin-hua1
With the rapid development of transgenic plant,the protection of species is becoming more and more important. The contents of wholesome elements and heavy metals in ten soybean species from northeastern China were studied by ICP-MS/CIP-AES to detect the heavy metals and microelements. The results showed that the Northeastern soybean contained many elements necessary to human health,the sequence of macroelements (higher than μg·g-1) was K>P>Mg>Ca>Fe>Rb>Mn≈Zn>Si≈Na≈Al≈Ba≈Ni≈Cu,and the most important is that the contents of Fe,Mn and Zn range from 20 to 80 μg·g-1,which are important to human health. Besides the microelements,the contents of heavy metals (As,Cr,Pb and Cd) are also the important standard to identify the quality of farm produce,and the results showed that northeastern soybean contained little heavy metals except Cr (near 200 ng·g-1). All the data showed that northeastern soybean accords with the national hygiene standards,but the protection should be strengthened.
2007 Vol. 27 (08): 1629-1631 [Abstract] ( 1765 ) PDF (339 KB)  ( 500 )
1632 Application of ICP-MS to Detecting Heavy Metals in Apple
ZHANG Hong-xing1,RUI Yu-kui2*
With the rapid development of the society,more and more attention has been focused on food′s edible safety,especially on the pollutions of heavy metals,pesticides and veterinary drug residues. Fuji apples bought from market were studied by ICP-MS to detect the heavy metals in peel and pulp. The results showed that the fruit pulp accumulated much less heavy metals (Cr，Sb，Cd，Pb，Sn，Zn，Cu，Co，Ni and Tl) than the fruit peel. All the data showed that heavy metals can pollute the fruit peel more easily than the fruit pulp,so with the pollution of environment the apple should be peeled before eating to protect our health. But the accumulating mechanism of heavy metals in fruit peel should be further studied.
2007 Vol. 27 (08): 1632-1633 [Abstract] ( 216 ) PDF (278 KB)  ( 525 )
1634 Determination of Trace Elements in the Sediments of Poyang Lake Basin by Microwave-Assisted-ICP-AES
GONG Xiao-feng1,2,CHEN Chun-li1,2,ZHAO Jin3,Barbara Zimmermann4,CUI Xiu-li1,ZHOU Wen-bin1*
In order to investigate the seasonal,annual and alongshore variation of the trace elements in the sediments of Poyang Lake in recent years,ICP-AES was used to determine the sediment of each sampling site collected in the year of 2003 and 2005 in different seasons.The results indicated that the contents of the elements in the sediments of Poyang Lake were changing with seasons and years. Generally,the content of each element in low-water period was more higher than in high-water period. Compared with the year of 2003,the contents of Cu and Pb at Nan Ji-shan were lower in the year of 2005,while Cai Jia-wan was in the reverse situation. The content of Cu at Yao Gong-du was also lower in the year of 2005,but Pb was higher than in the year of 2003. To some extent,the contents of Cu,Pb,Cr and Zn were higher than the background value of Poyang Lake basin. Except Dawu River,the content of As at other sampling sites was within the background value. From Raohe River to the Raohe River’s entry in Poyang Lake,the content of each element trended to decrease gradually. By using microwave-assisted-ICP-AES to determine the trace elements in the sediments of Poyang Lake,it was proved to be a simple and fast,efficient method.
2007 Vol. 27 (08): 1634-1637 [Abstract] ( 697 ) PDF (949 KB)  ( 510 )
1638 Contents of Li,Se,Mo and Cr in Bt Corns
HAO Yan-ling1,RUI Yu-kui1*,GUO Jing1,LUO Yun-bo1,HUANG Kun-lun1,2,ZHU Ben-zhong1
With the rapid development of the transgenic food，more and more transgenic food has been pouring into the market,raising concerns about transgenic food’s edible safety. Transgenic corns and their parents were scanned by ICP-MS to detect the contents of Li,Se,Mo and Cr. The results showed that the contents of Li,Se,Mo and Cr were much lower than those of their parents,especially the contents of Se and Mo in Bt corns were several times lower than their parents. All the results showed that the nutrients for human health could decrease due to the insertion of foreign genes,so transgenic should be strictly supervised before commercialization. And the molecular mechanism of the decrease in microelements should be further studied.
2007 Vol. 27 (08): 1638-1639 [Abstract] ( 1706 ) PDF (307 KB)  ( 503 )
1640 Determination of Trace Elements in Pollen by Using Atomic Absorption Spectrometry
LIANG Bao-an,FU Hua-feng
After the middle temperature cinefaction sample was dipped in 6 mol·L-1 HNO3,the relevant disturbance was removed by LaCl3 and CsCl,and the contents of ten elements(Cu,Fe,Mn,Zn,Pb,Cd,Ca,Mg,K and Na) were determined by flame atomic absorption spectrometry in the same solution by standard curve method. The experimental result indicates that there are abundant Zn,Mn,K,Ca,Na,Fe,Mg and Cu in the pollen,while the content of Pb is very low,and there is no Cd. Using the wild ageratum pollen as the sample,the proper condition of sample disposing and how to remove disturbance were studied and determined in detail,and the accuracy and precision of the method were examined. As a result,different element in the pollen doesn′t interfere with each other under the chosen condition. These ten elements can be determined in the same preparation solution respectively. The recovery is between 93.4％ and 112.0％,the relative standard deviation is between 0.3% and 2.6％ (n=5). The result is accurate and reliable.
2007 Vol. 27 (08): 1640-1643 [Abstract] ( 1732 ) PDF (449 KB)  ( 444 )
1644 A Novel Wavelet Multiple Thresholding Algorithm for Astronomical Spectral Signal Denoising
ZHAO Rui-zhen1,HU Zhan-yi2,HU Shao-hai1
By using the different relativities of spectral lines and noises in the wavelet domain,a novel wavelet multiple thresholding algorithm is presented in the present paper for astronomical spectra with low signal-noise-ratio (SNR). Firstly the wavelet coefficients are estimated by NeighShrink approach and then 0-1 coefficients are obtained. Based on the above binary coefficients,two kinds of relativity exponents at each scale and across scales respectively are defined for each wavelet coefficients. Finally decision coefficients are determined according to the magnitudes of the relativity exponents. This algorithm overcomes the over-reserving or over-shrinking disadvantages of the simple threshold method in that the decision coefficients are obtained by multiple criteria. Besides,large pulse noises can be removed by the presented algorithm because it takes spectral line features into consideration. The experimental results show that the proposed algorithm is computationally efficient and practical.
2007 Vol. 27 (08): 1644-1647 [Abstract] ( 1628 ) PDF (628 KB)  ( 541 )
1648 Auto-Extraction of Spectral Lines Based on Feature Constraints
LIU Rong1,DUAN Fu-qing2*,LIU San-yang1
By using single thresholding or local thresholding in spectral line recognition,nearly all methods for spectral line auto-extraction have the defect that there are many pseudo spectral lines or some spectral lines are lost. The present paper uses two feature constraints in spectral line recognition. The first constraint is that the central intensity of a spectral line must be higher than both the lower global threshold and the local threshold,and the point where the intensity is higher than both the upper global threshold must be on a certain spectral line. The second one is that the intensities at initial position and end position of a spectral line must be lower than its central intensity. The two feature constraints play a key role in improving the quality of spectral line extraction. Experiments show that this method is superior to the techniques used in the literature.
2007 Vol. 27 (08): 1648-1652 [Abstract] ( 1561 ) PDF (1395 KB)  ( 502 )
1653 Characteristics of Typical Optical Systems with Diffractive Gratings of Micro-Spectrometers and Improvement of Spectrometer’s Resolution
JIA Hui,YAO Yong
Many ways have been practiced in designing and fabricating micro spectrometer,each has its own characteristics distinguished by different spectral resolution and other performances. Micro spectrometers applied presently with high spectral resolution usually adopt optical systems with dispersive components being diffractive gratings. The development of micro spectrometer is reviewed briefly,and typical optical systems are analyzed and discussed,such as optical system based on Roland circle and that based on Czerny-Turner structure. The techniques and methods as well as the experiences of improving micro spectrometer’s spectral resolution are summarized,especially the tradeoff between miniaturization and spectral resolution,and the balance between spectral range and spectral resolution are considered. This summary gives a outline of the optical systems’ characteristic of dispersive micro-spectrometer,and it can be a reference for new micro spectrometer’s designing.
2007 Vol. 27 (08): 1653-1656 [Abstract] ( 1552 ) PDF (512 KB)  ( 512 )
1657 Test of the Effect of Different Supercritical Pressure on Andrographolide Crystallization with Chromatography and Spectrum
ZHANG Wen-cheng1,2,ZHANG Xing-yuan2,PAN Jian1
With the new technique of supercritical carbon dioxide extraction and crystallization,the experimental materials of 30% and 95% andrographolide were used to investigate the effect of different pressure on crystal distribution on crystallization board,what’s more,the effect of X-ray diffraction and infrared ray spectrum on crystal was tested. The results showed that andrographolide was crystallized on crystallization board in purity gradient with high performance liquid chromatography;the higher the pressure,the higher the crystallization ratio. In addition,the crystal was inclining to directional growth;the chemical structure of andrographolide was not changed with the variety of pressure with infrared ray spectrum analysis.
2007 Vol. 27 (08): 1657-1660 [Abstract] ( 2388 ) PDF (939 KB)  ( 475 )

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